超聲波輻照法制備三維貫通多孔碳整體柱畢業(yè)論文外文翻譯兩篇

1、附錄二 英文文獻(xiàn)與翻譯英文文獻(xiàn)13d interconnected macroporous carbon monoliths preparedby ultrasonic irradiationnattaporn tonanon , adisak siyasukh , yunyong wareenin ,tawatchai charinpanitkul , wiwut tanthapanichakoon , hirotomo nishihara ,shin r. mukai , hajime tamonabstract：a new method in preparation of 3d inte

2、rconnected macroporous carbon monolith has been introduced. ultrasonic irradiation(ultrasonic intensity 78 w/cm2) and low catalyst concentration (c/w = 10 mol/m3) of rf solution are used as an interesting and unique preparation method for 3d interconnected macroporous sonogel (gel irradiated by ultr

3、asound at gelation stage) and/or3d interconnected macroporous carbon monolith without using templates.keywords: porous carbon; pyrolysis; adsorption; scanning electron microscopy; porositymacroporous monolith is an interesting structure that has interconnected skeletons in a single column, and this

4、unique structure allows flow paths (throughpores)through the monolithic columns . carbon monolith has high potential to be good candidates for applications such as columns for chromatography, catalyst supports, adsorbents and porous electrodes under continuous flow conditions. macroporous carbon mon

5、oliths are mostly prepared by using carbon precursors and macroscopic shape templates . in general, macroscopic shape templates are interconnected skeleton such as silica template, zeolite, stable emulsions, polymer latex and the interstitial volume of other porous structures. carbon precursors are

6、polymeric materials or precursor of polymeric materials such as sucrose, some thermoplastics, phenolic resin, copolymerization of resorcinol fe(ii) complex and other thermosettings. there are some reports on macroporous carbon aerogels prepared by using metal catalyst or acid catalyst. in this work,

7、 a new method in preparation of 3d interconnected macroporous carbon monolith has been introduced. in general, ultrasonic irradiation has outstanding effects in many chemical reactions such as increasing reaction rates and yields of products, shortening reaction time, altering the reaction path and

8、making milder reaction conditions possible. an interesting role of ultrasonic irradiation on mesoporous properties of rf carbon gel when the ratio of catalyst to water c/w or ph is high was also reported 10. to the best of our knowledge, this study is the first to report on the work of ultrasonic ir

9、radiation (ultrasonic intensity 78w/cm2) together with low catalyst concentration (c/w = 10 mol/m3) of rf solution as an interestingand unique preparation method for 3d interconnected macroporous sonogel (gel irradiated by ultrasound at gelation stage) and/or carbon monoliths without usingtemplates.

10、macroporous sonogel monolith, precursors for macroporous carbon monolith, were prepared from resorcinol formaldehyde (rf) solutions which were composed of resorcinol (c6h4(oh)2) (r), formaldehyde (hcho) (f), sodium carbonate (na2co3) (c) and distilled water (w). all chemicals were research gradesfro

11、m wako pure chemical industries. na2co3 and distilled water were used as a basic catalyst and a diluent respectively. the ratios of resorcinol to formaldehyde (r/f), resorcinol to water (r/w) and catalyst to water (c/w) were fixed at 0.5 mol/mol, 8100 mol/m3 and 10 mol/m3 respectively. gelation temp

12、erature was 308 k. ultrasonic wave was applied into rf solution right from the start by vibra cell model vc 130 (frequency 20 khz) with a titanium alloy transducer at intensity 78 w/cm2. when it was close to the gelation time, the ultrasonic irradiation was stopped and the rf solution was then poure

13、d into the cylindrical glass tube (inner diameter = 3 mm, length = 40 mm) followed by aging for 7 days at 348 k in the oven. before freeze drying, water in rf sonogel monolith was replaced by solvent exchange with t-butanol for three times. after that, rf sonogels were freeze-dried at 263 k for 3 h

14、toobtain freeze dried macroporous rf sonogel monolith. macroporous carbon sonogel monoliths were obtained by pyrolyzing macroporous rf sonogel monoliths at 1023 k. pyrolysis was conducted under a 200 cm3stp/min flow of nitrogen gas. at first, the freezedried sonogels were heated to 523 k at a consta

15、nt heating rate of 523 k/h, and were kept at this temperature for 2 h.then they were heated to 1023 k at a constant heating rate of 523 k/h and were kept at 1023 k for 4 h.the structures of rf gel and rf sonogel monoliths were observed by scanning electron microscope(sem). macropore size distributio

16、n was measured by using mercury porosimeter. porous properties, bet surface area (sbet), mesopore volume (vmes) and micropore volume (vmic), were determined from the n2 adsorption method using an adsorption apparatus.the effect of ultrasonic irradiation at gelation stage can be seen as followed. in

17、gelation process, gelation time is shortened outstandingly with ultrasonic irradiation. gelation time obviously decreases from 48 h (rf gel monolith) to 8 h (rf sonogel monolith). the shrinkages of 3d interconnected macroporous rf gel monolith and rf sonogel monolith, after freeze drying, are 21% an

18、d 1% respectively. it is obvious that ultrasonic irradiation leads to small shrinkage in rf gel sonogel monolith compared to rf gel monolith. in fig. 1, the cross section of rf sonogel monolith observed by sem shows 3d interconnected macroporous structure which is totally different from mesoporous s

19、tructure of rf gel monolith. sbet are 228 (rf gel monolith) and 5 (rf sonogel monolith) m2/g. vmic and vmes of rf gel are 0.02 and 0.32 cm3/g respectively. for rf sonogel monolith, vmic and vmes cannot be detected.after pyrolysis of rf sonogel monolith, no change in macroporous structure and very lo

20、w shrinkage are observed.after pyrolysis sbet and vmic of sonogel increases from 5 to 366 m2/g and n/d to 0.11 cm3/g respectively (vmes cannot be detected). it can be seen from sem micrograph in fig. 2 together with porous properties that rf carbon monolith can keep 3d interconnected macroporous str

21、uctures. the macropore size distributions of carbon monolith are narrow, the average macropore size around 13 lm as shown in fig. 3. in this work, new synthesis method for 3d interconnected macroporous sonogel and/or carbon monolith is proposed with some advantages to other methods such as shorter g

22、elation time of polymer monolith, small shrinkage percentage, no template preparation and template removal. in addition to this preliminary work, the effect of r/c on the structure of 3d interconnected macroporous carbon monolith (microwave drying at 200 w after solventexchange with t-butanol) has b

23、een investigated. in figs. 4 and 5, r/c = 1200 mol/mol gives 3d interconnected macroporous carbon monolith with smaller pore diameters than r/c = 800 mol/mol. 3d interconnected macroporous carbon monolith from both r/c = 800 and 1200 mol/mol show narrow pore size distributions as shown in fig. 5. it

24、 is obviously seen that r/c has effects on the structure of interconnected macroporous carbon monolith. these results suggest that there is a possibility to tailor pore structure of 3d interconnected macroporous sonogel monolith (precursor of 3d interconnected macroporous carbon monolith) directly a

25、nd effectively at gelation stage with suitable reactant ratios of rf solution and ultrasonic intensity.references1 tanaka n, kobayashi h, nakanishi k, minakuchi h, ishizuka n. a new type of chromatographic support could lead to higher separation efficiencies. anal chem 2001:421a9a.2 liang c, dai s,

26、guiochon g. a graphitized-carbon monolithic column. anal chem 2003;75:490412.3 taguchi a, smatt jh, linden m. carbon monoliths possessing a hierarchical, fully interconnected porosity. adv mater 2003;15:120911.4 shi zg, feng yq, xu l, da sl, zhang m. synthesis of carbon monolith with trimodal pores.

27、 carbon 2003;41:265389.5 bu h, rong j, yang z. template synthesis of polyacrylonitrilebased ordered macroporous materials and their derivatives. macromol rapid commun 2002;23:4604.6 kang s, yu js, kruk m, jaroniec m. synthesis of an ordered macroporous carbon with 62 nm spherical pores that exhibit

28、unique gas adsorption properties. chem commun 2002:16701.7 peters ec, svec f, frechet jmj. rigid macroporous polymer monoliths. adv mater 1999;11:116981.8 moreno-castilla c, maldonado-hoda fj, rivera-utrilla j, rodrguez-castellon e. group 6 metal oxidecarbon aerogels. their synthesis, characterizati

29、on and catalytic activity in the skeletal isomerization of 1-butene. appl catal a 1999;183:34556.9 brandt r, petricevic r, probstle h, fricke j. acetic acid catalyzed carbon aerogels. j porous mater 2003;10:1718.10 tonanon n, siyasukh a, tanthapanichakoon w, nishihara h, mukai sr, tamon h. improveme

30、nt of mesoporosity of carbon cryogels by ultrasonic irradiation. carbon 2005;43:52531.11 suslick ks, price gj. applications of ultrasound to materials chemistry. annu rev mater sci 1999;29:295326. 翻譯1超聲波輻照法制備三維貫通多孔碳整體柱nattaporn tonanon, adisak siyasukh , yunyong wareenin ,tawatchai charinpanitkul ,

31、wiwut tanthapanichakoon , hirotomo nishihara ,shin r. mukai , hajime tamon摘要:介紹一種制備三維貫通多孔碳的新方法。間苯二酚-甲醛溶液在超聲波輻照(超聲波強(qiáng)度78w/cm2)和低催化劑濃度（c/w=10mol/m3）下制備三維貫通多孔聲致凝膠(凝膠在膠化階段輻射超聲波) ，是目前倍受關(guān)注的也是唯一的一種不用模板的多孔碳整體柱的制備方法。關(guān)鍵詞：多孔碳 熱分解 吸附 掃描電鏡 孔隙率在一個(gè)單獨(dú)柱體內(nèi)具有連通骨架的多孔整體柱是一個(gè)受關(guān)注的結(jié)構(gòu)，并且這種唯一的結(jié)構(gòu)能夠貫通整個(gè)整體柱。碳整體柱因?yàn)榫哂泻芨叩膭?shì)能作為整體柱便于應(yīng)用

32、于色譜分析，催化劑支架,吸附劑和多孔電極具有連續(xù)不斷的流動(dòng)條件。多孔碳整體柱大部分都是用碳前驅(qū)體和宏觀外形的模板制備的。大體上講，宏觀外形的模板都具有連通的骨架像硅模板，沸石，穩(wěn)定的乳劑，高分子乳膠和具有空隙的其它結(jié)構(gòu)。碳前驅(qū)是聚合材料或是聚合材料前驅(qū)像蔗糖，一些熱塑性材料，酚醛樹脂，間苯二酚fe()絡(luò)合物的共聚物和其它熱固性的材料。有一些關(guān)于利用金屬催化劑或者酸催化劑制備多孔碳?xì)饽z的報(bào)道。本文介紹了一種制備三維連通多孔碳的新方法。大體上講，超聲波輻射法在許多化學(xué)反應(yīng)像提高反應(yīng)速率與提高反應(yīng)產(chǎn)率，縮短反應(yīng)時(shí)間，修改反應(yīng)途徑和使反應(yīng)條件盡量溫和中是比較優(yōu)異的方法。超聲波輻射法一種受關(guān)注的在中孔

33、材料性質(zhì)中催化劑與水的比例或者ph過高的作用也有人報(bào)道過。具我所知，這篇文章是第一篇報(bào)道關(guān)于rf溶液中的超聲波輻射(超聲波強(qiáng)度78w/cm2)和低催化劑濃度（c/w=10mol/m3）是前一段時(shí)間受關(guān)注的也是唯一的一種制備無模板整體柱三維連通多孔聲致凝膠的一種方法(凝膠在膠化階段照射超聲波)。多空聲致凝膠整體柱是多孔碳整體柱的前驅(qū)，是從由間苯二酚(c6h4(oh)2)(r),甲醛（hcho）(f)，固體碳酸鈉（na2co3）(c)和蒸餾水（w）組成的（rf）溶液中制備的。所有的化學(xué)用品都是從wako pure化學(xué)公司研究開發(fā)的。na2co3和蒸餾水分別被用作基本催化劑和稀釋劑。間苯二酚和甲醛的

34、比例（r/f），間苯二酚和蒸餾水的比例(r/w)和催化劑與蒸餾水的比例（c/w）是固定的分別是0.5mol/mol，8100mol/m3和10mol/m3。膠化溫度為308k。超聲波被應(yīng)用到rf溶液中，它正好是由78 w/cm2強(qiáng)度的鈦合金傳感器組成的震動(dòng)電池模型vc130（頻率為20khz）發(fā)揮作作用的。當(dāng)它接近凝膠時(shí)間時(shí)，超聲波就會(huì)停止，rf溶液然后被倒入圓柱形的玻璃試管（該試管內(nèi)部直徑是3mm, 長40mm）,在348k的烘箱內(nèi)烘烤7天。在低溫干燥之前，在rf聲致凝膠整體柱內(nèi)的水應(yīng)與叔丁醇進(jìn)行3次溶劑交換。在這之后，rf聲致凝膠低溫干燥在263k下干燥3小時(shí)獲得低溫干燥的多孔rf聲致凝膠

35、整體柱。多孔碳聲致凝膠整體柱是由多孔rf聲致凝膠整體柱在1023k下高溫分解而得的。熱分解在200cm3stp/min的氮?dú)獗Ｗo(hù)下進(jìn)行的。首先，低溫干燥聲致凝膠在523k/h的速度下加熱到523k，并保溫2h。再以523k/h的速度加熱到1023k保溫4h。rf凝膠和rf聲致凝膠整體柱的結(jié)構(gòu)是利用掃描電鏡（sem）進(jìn)行觀測(cè)的。多孔的尺寸和分布是利用汞孔隙率計(jì)測(cè)量的。多孔的性質(zhì)，比表面積（sbet），孔隙體積（vmes）和小孔體積（vmic），是利用吸附儀器測(cè)n2的吸附量的方法測(cè)定的。在膠凝階段超聲波的作用可以在下面看出。在膠凝過程中，超聲波使膠凝時(shí)間顯著縮短。膠凝時(shí)間明顯的從48h（rf凝膠整

36、體柱）減少到8h（rf凝膠整體柱）。在低溫干燥后，三維連通多孔rf凝膠整體柱和rf聲致凝膠整體柱的收縮率分別為21和1。由超聲波導(dǎo)致rf聲致凝膠整體柱的收縮比rf凝膠整體柱要小。如圖1，通過掃描電鏡觀測(cè)到的rf聲致凝膠整體柱的三維連通多孔結(jié)構(gòu)與rf凝膠的中孔結(jié)構(gòu)完全不同。sbet分別為228m2/g（rf凝膠整體柱）和5 m2/g（rf聲致凝膠整體柱）。rf凝膠的vmes 和vmic分別為0.02 cm3/g和0.32cm3/g。rf聲致凝膠整體柱的vmes 和vmic測(cè)不出。 圖1:rf凝膠和rf聲致凝膠整體柱 圖2：rf碳整體柱的sem的sem顯微照片（橫截面在1000） 顯微照片（橫截面

37、在1000）聲致凝膠整體柱熱解后，觀測(cè)到的多孔結(jié)構(gòu)和比較低的收縮率沒有發(fā)生變化。熱解后的聲致凝膠的sbet從5 m2/g變到366 m2/g，vmic變到0.11cm3/g（vmes 測(cè)不出）從圖2的sem的顯微照片可以看出具有多孔性質(zhì)的rf碳整體柱能保持三維連通多孔結(jié)構(gòu)。碳整體柱的尺寸分布比較小，從圖3可以看出平均孔徑大概是13m。這篇文章，合成三維連通多孔聲致凝膠和碳整體柱的新方法優(yōu)于其它方法主要在于縮短了高分子整體柱的膠凝時(shí)間，具有較小的收縮百分比，無模板制備和樣板移動(dòng)。 圖3：rf碳整體柱的多孔尺寸分布 圖5：rf碳整體柱的多孔尺寸分布 （c/w=10 mol/m3，微波干燥）圖4：r

38、f碳整體柱的sem顯微照片（c/w=10 mol/m3，微波干燥）在前期工作的基礎(chǔ)上，我們研究一下r/c對(duì)三維連通多孔碳整體柱（微波干燥是在200w的條件下進(jìn)行與叔丁醇的溶劑交換）的結(jié)構(gòu)的影響。從圖4和圖5可以看出r/c=1200mol/mol時(shí)得到的三維連通多孔碳整體柱的孔直徑要小于r/c=800mol/mol時(shí)得到的三維連通多孔碳整體柱。從圖5可以看出r/c800mol/mol和r/c=1200mol/mol的三維連通多孔碳整體柱都具有較小的孔尺寸分布?？梢钥闯鰎/c對(duì)連通多孔碳整體柱的結(jié)構(gòu)有著明顯的作用。這些結(jié)構(gòu)證明我們可以直接有效的在膠化階段配以合適的rf溶液與超聲波的比例來控制三維連

39、通多孔聲致整體柱（的三維連通多孔碳整體柱的前驅(qū)）的孔結(jié)構(gòu)。參考文獻(xiàn)：1 tanaka n, kobayashi h, nakanishi k, minakuchi h, ishizuka n. a new type of chromatographic support could lead to higher separation efficiencies. anal chem 2001:421a9a.2 liang c, dai s, guiochon g. a graphitized-carbon monolithic column. anal chem 2003;75:490412.3

40、taguchi a, smatt jh, linden m. carbon monoliths possessing a hierarchical, fully interconnected porosity. adv mater 2003;15:120911.4 shi zg, feng yq, xu l, da sl, zhang m. synthesis of carbon monolith with trimodal pores. carbon 2003;41:265389.5 bu h, rong j, yang z. template synthesis of polyacrylo

41、nitrilebased ordered macroporous materials and their derivatives. macromol rapid commun 2002;23:4604.6 kang s, yu js, kruk m, jaroniec m. synthesis of an ordered macroporous carbon with 62 nm spherical pores that exhibit unique gas adsorption properties. chem commun 2002:16701.7 peters ec, svec f, f

42、rechet jmj. rigid macroporous polymer monoliths. adv mater 1999;11:116981.8 moreno-castilla c, maldonado-hoda fj, rivera-utrilla j, rodrguez-castellon e. group 6 metal oxidecarbon aerogels. their synthesis, characterization and catalytic activity in the skeletal isomerization of 1-butene. appl catal

43、 a 1999;183:34556.9 brandt r, petricevic r, probstle h, fricke j. acetic acid catalyzed carbon aerogels. j porous mater 2003;10:1718.10 tonanon n, siyasukh a, tanthapanichakoon w, nishihara h, mukai sr, tamon h. improvement of mesoporosity of carbon cryogels by ultrasonic irradiation. carbon 2005;43

44、:52531.11 suslick ks, price gj. applications of ultrasound to materials chemistry. annu rev mater sci 1999;29:295326.英文文獻(xiàn)2a new methodto estimate pore volume of porousstyrenedivinylbenzene copolymersmuhammadarif malik , munir ahmed, muhammad ikramabstract：a new method to estimate the pore volume of

45、porous styrenedivinylbenzene copolymer beads is proposed.the estimatedpore volume（pve）is basedon the solubility parameters （i） andthe corresponding weight fractions（fi） of styrene, divinylbenzenes and diluents in the polymerization mixture. the equation used is: pve=1.136（i fi）231.193i fi98.825. reg

46、ression analysis results show that an ideally close match of the predicted pore volume andthe pore volume determined by mercury porosimeter is achievedwith r2=0.99, when non-polar and moderately polar liquids are employed as diluents. in the case of strongly polar (h-bonding) liquids as diluents, th

47、e method should be used only to predict a trend towards an increase or decrease in pore volume, which occurs as a result of variation in the composition of polymerization mixture.keywords: styrene-divinylbenzene; pore volume estimation; solubility parameters; macroporous resins; polymeric adsorbents

48、1. introductionporous styrenedivinylbenzene (s-dvb) copolymer beads are produced on an industrial scale as well as in laboratories throughout the worldby o/w suspension polymerization andthen convertedto ionexchangers,chelating resins, supports for catalysts and enzymes, etc. . the monomers are dilu

49、ted with some inert organic liquidthat introduces porosity in the copolymer . the porosity is determined by amount andsolvating property of the diluents andthe degree of cross-linkage in the copolymer . this has been a subject of research interest in the past 50 years, as is evident from review arti

50、cles published from time to time , and some recent research articles .porous copolymers from a number of relatedmonomers have also been synthesizedby the same technique, e.g., methacrylamide t styrene divinylbenzene , acrylonitriledivinylbenzene , glycidyl methacrylateethyleneglycol dimethacrylate ,

51、 methacrylic acidtriethyleneglycol dimethacrylate , acrylic acidtriethyleneglycol dimethacrylate, acrylamideethyleneglycol dimethacrylate , 4-vinylpyridinedivinylbenzene, etc.some important properties of the derived products depend on the porous structure of the s-dvb base copolymer . pore volume is

52、 an important parameter that is relatedto the porous structure of the copolymer. the pore volume in the dry state of the copolymer is usually determined by nitrogen desorption(bet) or mercury penetration methods. these methods require expensive instruments. we have proposeda simple, inexpensive, yet

53、 reasonably accurate methodof pore volume determination, which is based on the density of the dried copolymer beads . here, we propose a simple empirical relation which can be usedto pre-determine pore volume of the s-dvb copolymers before they are actually produced. the relation will be helpful in

54、deciding the appropriate composition of thepolymerization mixture requiredfor obtaining a copolymer of desired porosity.2. experimentalsolubility parameter （） values of liquids (in hildebrandunit (h) were taken from the crc hand book. when the value was not listedin the reference, it was calculatedb

55、y using the following formula: （d（hvrt）/m）1/2 (where d，hv and m are density, heat of vaporization andmolecular weight, respectively, for the liquidand r and t are gas constant andabsolute temperature, respectively, taken from ref. ). the solubility parameter can also be estimatedbasedon the group co

56、ntribution methodof hoftyzervan krevelen andthe methodof hoy . the d values of styrene, divinylbenzene and diluent/s were multipliedwith their corresponding weight fraction（fi） in their mixture andsummedto get i fi. a sample of pore volume values, determined by mercury porosimetry （pvm）andreportedby

57、 different research groups at different times, was taken from the published literature. the pvm values were plottedas a function of pdifi and a second-degree polynomial was fittedto the data using microsoft excel software in the form: pve=a（i fi）2bi fic. in this equation, pve is the pore volume esti

58、matedby the best-fit equation and a, b and c are the constants determining the shape of the curve.some s-dvb copolymers were synthesizedto experimentally verify the proposedpore volume estimation method. styrene, divinylbenzenes (comprising of 60% divinylbenzene isomers and 40% ethylvinylbenzene isomers)andd iluents were mixedat 26.6%, 13.3% and 60% ratio by volume, respectively. benzoylperoxide (1% by weight) was dissolved in the mixtur